関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Urea | HCID 1176 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 反応物 | 2-(3,4-Dichlorophenoxy)-3-(dimethylamino)prop-2-enal | HCID 54555818 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178517841 | HCID 178517841 | 17.3% |
反応手順
A solution of sodium ethoxide, prepared from sodium (0.95 g, 41.4 mmol), 2-(3,4-dichlorophenoxy)-3-dimethylamino-propenal (5.38 g, 20.7 mmol) and urea (2.48 g, 41.4 mmol) in ethanol (25 ml) was heated at 60° C. for 4 hours. Water (1 ml) was added and heating was continued for an additional 2 hours. The solution was cooled to room temperature and neutralised with glacial acetic acid. Most of the solvent was removed by evaporation in vacuo. Water was added and the precipitate was isolated by suction, followed by drying in a vacuum oven, yielding the title compound (0.92 g, 17% yield) as a brown solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07279470B2 |
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| 出典データセット | uspto-grants-2007_10 |
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| ORD ID | ord-013cd658c52c4729b497545a849f88cd |
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| 出典メモ | uspto-grants-2007_10 |
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